C&EN Whitepapers

C&EN Whitepapers

Inexpensive compact mass spectrometers are expected to continue their charge into university teaching laboratories, where their speed, usability and robustness are enabling – in many cases, for the first time – undergraduate students to have hands-on experience with an instrument that they are increasingly likely to encounter if they progress through a scientific career.

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Aqueous colloidal silica, essentially made of just sand and water, is turning up in surprising ways at the forefront of research. A new collection of case studies highlights some of the exciting ways academic researchers are using colloidal silica to expand the frontiers of materials science. Nano-zeolites, bijels, and soft robots are among the novel applications featured in this new ebook: “Colloidal Silica: Small Particles, Enormous Potential”.

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Automation in chemistry can repeatably and reliably perform chemical reactions at a reduced reaction scale. These attributes enable the researcher to explore a larger set of chemical reaction conditions for DoE, solubility, reaction screening and process optimization to name a few. We present five examples of how automation solutions from Unchained Labs can be used by chemists to more thoroughly, quickly, and efficiently discover new reaction paths and conditions.

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Adhesives are indispensable in the automotive, aeronautic, and medical industries, among others. Modern adhesives are complex, and their quality requires an assessment of initial components as well as the final product. Molecular spectroscopy approaches, including FTIR and Raman, can be used to identify the components of a sample within seconds without any sample preparation, reagents, or consumables, offering a fast and effective route to glue analysis. Microspectroscopy can detect defects and inclusions on adhesive surface, while confocal Raman microscoscopy provides a unique capability: to analyze materials in depth without the need for a cross-section.

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As pharmaceutical companies have shifted their development focus to large-molecule biotherapeutics, the ability to separate intact monoclonal antibodies and antibody-drug conjugates for characterization purposes has become extremely important. To enable this characterization work, new LC particle technology has been required. The large 1000 Å pore size of the superficially porous particles used for RPLC described herein enables full access to the bonded phase surface for larger biomolecules. This improved access to the bonded surface produces narrower peak widths and enhanced resolution of minor mAb variants, and can lead to increased retention under most analysis conditions. Together, with new mass spectrometric instrumentation and software, wide-pore superficially porous particle LC columns will greatly aid in the advancement of large-molecule biopharmaceutical characterization and development. The recent expansion of the very large pore superficially porous particle family to include three bonded phases (C4, C18, Diphenyl) permits very high resolution separations of lower abundance protein variants, permitting structure analysis and quantification of these variants.

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This whitepaper aims to provide pharmaceutical researchers a better understanding of the uses and benefits of hybrid silica-based supports in HPLC separations of drug compounds. In a quick, absorbing read that includes commentary from a number of experts in the field, readers can find out how hybrid silica-based chromatography rose to popularity in the pharma lab, and why. The many benefits of hybrid silica materials are compared and contrasted with traditional silica usage, supported by references and examples from end users.

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Identification and quantification of impurities in pharmaceuticals is critical throughout drug development and manufacture to ensure product quality. There are significant risks when using a qualitative certified reference standard for a quantitative analysis. Learn how the characterization of reference standards can dramatically reduce the risk of out of specification investigations, lengthy toxicity studies, and even the loss of entire batches.

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Crystallization of active pharmaceutical ingredients is critical to the successful development and manufacture of medications. However, crystallization challenges are common and can negatively affect pharmaceutical development and complicate regulatory filings. This whitepaper identifies strategies to overcome those challenges to meet the demands of today’s pharmaceutical industry.

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A successful high-throughput approach to reaction screening requires a rational and systematic exploration of a broad set of variables to achieve optimization. Even with the aid of high-throughput screening tools, it’s still unlikely that all the possible combinations of reaction variables a process chemist desires can be screened. A well-planned high-throughput approach enables scientists to more clearly see the “big picture,” quickly abandon suboptimal strategies, and rapidly pinpoint advantageous conditions.

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Increased peak capacity provided by the TIMS technology coupled to a QTOF mass spectrometer and the PASEF acquisition mode together with novel chromatographic separation technology provides beneficial separation to analyze 200 samples per day. The high speed of the new mass spectrometer enables measurement at sufficient analytical depth and robustness and is ideally-suited for the measurement of large sample cohorts.

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Chemical manufacturing such as polyurethane production is characterized by a cost intensive production process combined with a negative ecological impact. These adverse effects can be significantly improved by using vibrational spectroscopy. This analytical technique can assist the operator of the plant to reduce costs and minimize the impact on the environment.

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Monoclonal antibody (mAb) therapeutics have been widely used to treat various diseases, including cancer. Oftentimes, dimers and other high molecular weight aggregates are present in the mAb therapeutics, leading to reduced biological activity. Traditionally-used methods for aggregate removal rely heavily on anion exchange chromatography (AEX) in flow-through mode followed by a generic bind/elute polishing step. While there are several advantages associated with these methods, they are often time-consuming and expensive. This whitepaper reports the use of hydrophobic interaction chromatography (HIC) in lieu of the generic bind/elute polishing step, for the removal of aggregates from mAb therapeutics. HIC is a more simple and cost-effective method, leading to higher selectivity towards mAb aggregate removal.

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Pharmaceuticals play a prominent role worldwide. This widespread presence is met with regulatory requirements at each phase of pharmaceutical development and manufacturing—from inspection of raw materials to quality control of final products. Consistently producing pharmaceuticals that both continue to satisfy the consumer and adhere to regulatory mandates, requires analytical methods, instruments, and systems that ensure quality standards are upheld throughout the pharmaceutical industry. In the following chapters, you will discover relevant analytical techniques, useful industry examples, and tips for assuring continued compliance with the latest regulations.

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A surprisingly large number of materials have unpaired electrons. These include free radicals, many transition metal ions, and defects in materials. Free radicals are often short-lived, but play crucial roles in many significant processes such as photosynthesis, oxidation, catalysis, and polymerization reactions. Electron paramagnetic resonance (EPR) spectroscopy is the only method for the direct detection of species that have unpaired electrons, and its applications span one of the widest ranges of any analytical technique.

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In this study the Toxtyper is used for drug screening in drug consumption rooms which are seen as an important element to minimize drug-related health problems (e.g. infection risk) and promote contact of drug users with employees of drug help programs.

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The use of microbial fermentation to make biologics is growing rapidly. A manufacturing platform is an increasingly popular way to speed up process development stages and get a biologic to market faster. High-throughput systems can speed up optimization of each of these platform steps. Single-use, disposable technologies are starting to replace stainless steel to streamline biologic manufacturing, reduce costs, minimize contamination risks and allow rapid expansion of capacity.

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The genome has given clinical researchers a powerful tool for understanding the biological foundations of many diseases, but it only tells part of the story. This ebook shows how different laboratories are employing mass spectrometry and other cutting-edge tools to collect richer datasets based on a combination of multiple ‘omes’, including the proteome, metabolome and transcriptome. Through the integrated analysis of these molecular profiles, researchers can glean insights that would be impossible to obtain with any one dataset alone—for example, the mutations in the genome can be a poor predictor of actual gene expression or protein production. The case reports presented in this collection show how these multi-omic analyses can potentially lead to earlier and more accurate research predications, and ultimately, to possible individualized treatment regimens.

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This study describes a new method of quantifying different types of microplastics in environmental samples using FTIR imaging. The method utilized was able to successfully recover, identify, and quantify microplastics in organic-rich samples such as sediment, water, and fish. The method utilized FTIR imaging, combined with the MPhunter software and proved to be a rapid and accurate way to automatically identify and quantify microplastics and other materials. Combined with H2O2 oxidation, FTIR imaging is a strong candidate to be a standard method in microplastic analysis, allowing further study and understanding of microplastics in the environment.

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There are currently a half-dozen different insulin analogues on the market. These differ from each other and from natural insulin by just a few amino acids, but exhibit markedly different pharmacokinetic and pharmacodynamic properties. Liquid chromatography and mass spectrometry (LC-MS) offers a powerful tool for the sensitive and quantitative detection and discrimination of these highly similar recombinant proteins. This whitepaper reviews the considerations that analytical chemists should take into account when planning to undertake LC-MS analysis of an insulin analogue-containing specimen.

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As plastics continue to enter the environment, understanding their global impact is vital to addressing microplastic pollution. Since its emergence as an environmental and potential human health threat, researchers have strived to develop tools for accurately measuring microplastics in environmental and food matrices using FTIR-based techniques and automated data handling. This study examines the current status of methods of microplastic quantification and identification and presents the analysis of microplastics smaller than 10 microns in a sample of soil from a marina using FTIR imaging, combined with a free software program, MPhunter.

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A drug discovery research project can be made more efficient, with reduced costs and increased likelihood for success, through optimal handling of the diverse information the project generates. The discovery team is inherently data driven, and the volume of data generated is often overwhelming, discipline-specific, and difficult to interpret. Modern informatics systems can help make that data conveniently available, and user friendly visualization renders it readily interpretable by all members of the project team.

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Chemists working in academic research, industry, and non-profit organizations alike face mounting challenges in data management. C&EN and software provider ACD/Labs commissioned a survey to better understand how laboratories currently manage their analytical data. Do researchers feel they are able to adequately manipulate, share, and retrieve data? Are they confident in data accuracy?

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In this white paper, it will be demonstrated that the use of three HILIC phases, which provide very different and complementary selectivity to one another, is both practical and effective for HILIC method development. These selectivity differences can be exploited, together with mobile phase pH, to thoroughly explore selectivity and to enable selection of an appropriate stationary phase/mobile phase combination during HILIC method development. A systematic, step-by-step approach to method development is recommended to make it easier for chromatographers to develop new HILIC methods in a productive manner.

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Hydrogen peroxide and peracetic acid are versatile oxidizing agents that combine powerful oxidation with exceptional environmental compatibility. Their bona fide green chemistry credentials should help every modern chemist appreciate their potential applications. This comprehensive ebook delves into the myriad applications for hydrogen peroxide and peracetic acid, with chapters highlighting their role in chemical synthesis, aseptic packaging, and environmental applications such as wastewater treatment. This ebook can be downloaded in its entirety or as individual chapters. The chapters cover the roles of hydrogen peroxide and peracetic acid in chemical synthesis, aseptic packaging and wastewater treatment. Please choose if you would like to download the entire ebook or one of the chapters.

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This white paper highlights six key points that pharmaceutical and biotechnology companies should keep in mind when looking to select the ideal partner to synthesize an API for them—and ensure their drug development process stays on the path to success.

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The whitepaper describes the latest advances in methods, hardware, and software for intact mass analysis. It desribes how these advances could be combined to further push the boundaries for intact mass analysis for complex heterogenous biologic samples.

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This whitepaper explores how LC/MS analysis of intact therapeutic antibodies can be performed with high accuracy and sensitivity down to subnanogram levels for molecular weight confirmation and assessment of isoform pattern. For the analysis of more complex molecules, such as antibody-drug conjugates, native mass spectrometry is beneficial to characterize the sample and obtain the accurate drug-to-antibody ration.

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Liquid chromatography and mass spectrometery (LC-MS) have transformed the field of proteomics, enabling researchers to rapidly survey the contents of complex biological samples. However, until relatively recently it has proven challenging and labor-intensive to perform accurate comparisons across multiple samples.

Tandem mass tags (TMT) have proven to be a transformative tool in this regard. Using TMT technology, researchers can add isobaric labels to multiple samples, which can then be analyzed in a single tandem MS experiment. These capabilities are making it possible to sensitively detect rare peptide species, to identify differences between healthy and diseased tissue, and conduct sophisticated surveys of the cellular proteome. This ebook provides an overview of the TMT technology, and offers five case studies that illustrate some of the cutting-edge applications for which these reagents are being used.

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The dominant technology of modern proteomics is certainly liquid chromatography-mass spectrometry (LC-MS). However, it is safe to say that the primary discussion point in terms of technology in proteomics has been the mass spectrometry part of this partnership. A great deal of emphasis is placed on the mass spectrometer and the data generated by it.

However, there has been less focus and emphasis placed on the separations of peptides and proteins prior to analysis by mass spectrometry in terms of the nano-LC chromatography systems and columns contributing to proteomics performance. One half of the LC-MS combination has been neglected.

Therefore it seemed to the authors that it was time this imbalance was redressed. The following handbook has been produced in an attempt to educate and inform on the relevance and significance to proteomics of liquid chromatography, in particular reversed-phase nano-LC directly coupled to MS.

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Compact mass spectrometers (CMS) have revolutionized reaction monitoring, turning a once laborious and time-consuming task into a rapid and convenient process with instruments right at the chemist's bench or fume hood. These instrument can provide results in as few as 30 seconds, are cost-effective, and offer a growing number of sample techniques. This report reviews the advantages and applications of CMS systems as well as some case studies in their use.

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The coatings industry, just like every other segment of the chemical industry, is innovating in response to new and expanding environmental regulations. As one of the world's biggest users of chemical ingredients, coatings manufacturers are under intense pressure to meet new standards but also provide affordable and efficient products. Innovative companies have responded with new additives that help achieve goals such as reducing levels of hazardous air pollutants (HAPs) and volatile organic compounds (VOC), as well as making certain that coatings that come in contact with foods are up to today's safety standards.

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Compact mass spectrometers (CMS) have revolutionized reaction monitoring, turning a once laborious and time-consuming task into a rapid and convenient process with instruments right at the chemist's bench or fume hood. These instrument can provide results in as few as 30 seconds, are cost-effective, and offer a growing number of sample techniques. This report reviews the advantages and applications of CMS systems as well as some case studies in their use.

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From protein folding to the function of medicines in the body, water is essential to countless chemical reactions that sustain life. Recently, the advent of liquid cell transmission electron microscopy has brought these tiny interactions to light with high-resolution imaging. Using customizable sample holders, researchers are now performing water-based science experiments inside the electron microscope.

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Homogeneous, assembled, digitized analytical data lends itself to be included in the stream of meaningful data exchange between external organizations and data-sharing inside organizations. This organization and data transformation is necessary to effectively build the ‘data-to-information-to-knowledge’ lineage that enables managers to make strategic and tactical decisions; to maximize benefits, and limit risks. This paper provides commentary on efforts for analytical data standardization and a vision of the broader considerations and requirements that such an undertaking should include.

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Ongoing evolution of new designer drugs, also known as new psychoactive substances (NPS), requires continuous updating of screening methods when determining the suspected role of NPS in deaths. The open library concept of the Toxtyper system allows for rapid updates of methods linked to the appearance of new drugs.

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Increases in regulatory scrutiny on consumer safety, shifts in popular perception and the urgency to stay in front of chemical resistance curves all impact the agricultural chemicals industry. Meanwhile, food demands increase as the global population continues to soar. Modern agricultural chemicals R&D teams are under more pressure than ever to deliver cutting-edge synthetic pesticides, herbicides and fertilizers to market while balancing regulatory, social and technical demands.

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For many years pharmaceutical companies have taken a deliberate approach for creating new small molecule drugs for disease treatment. These new chemical entities and their analogs were often synthesized in large numbers and then tested for efficacy for treatment of various diseases…

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Analytical testing across the broad commercial range of consumer products is essential to ensure the safety of end users, support the continuous supply of quality offerings to the marketplace, protect a company’s brand and reputation,and meet regulatory requirements...

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Genotoxic impurities (GTIs) are intermediates or reactants that can develop during the synthesis of a drug substance. In addition to process impurities, certain drugs may generate GTIs via degradation during formulation or storage...

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The agrochemicals industry has come under increasing pressure to bring to market new, less costly, and highly effective crop protection products with reduced environmental footprint compared to traditional herbicides and pesticides...

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Measuring viscosity is a tried and true technique for characterizing fluids. But frequently viscosity measurements are not made correctly and accordingly do not provide reliable or meaningful information...

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The pharmaceutical and biopharma industry continues to experience solid growth in an expanding global market. This market growth has been accompanied by an ever-changing industry landscape, with consolidation among long-time "big pharma" leaders, ongoing mergers and acquisitions, and the emergence of start-ups and technology-based offshoots from academic laboratories...

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The emergence of new and increasingly complex synthetic biopolymers, novel polymers, and polymer additives with a broad range of structural and compositional diversity has been a driving force in the development of advanced separation and analytical technologies for polymer characterization...

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End-to-end automation of an integrated liquid chromatography-mass spectrometry (LC-MS) workflow for target screening applications is readily achievable and yields substantial advantages...

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Laboratory based organizations face a wide variety of unaddressed data management challenges, and yet ultimately their scientific data is the currency with which they trade...

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There is growing need for research groups to adopt a Laboratory Information Management System (LIMS). A reliable, flexible and easy-to-use LIMS is an increasingly essential research tool that enables...

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Proteomics techniques are rapidly evolving to become a highly sensitive, quantitative, and high-throughput approach to analyzing global protein dynamics within a cell, tissue or an organism...

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Cannabis testing is a rapidly growing business expected to exceed $8 billion in 2017. It is fueled by many factors including consumer demand, evolving legislation, and growing evidence of the benefits of medical marijuana, which is now legal in 23 states and the District of Columbia...

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Manufacturers of pharmaceuticals, drug delivery systems, and biomedical devices have come under growing pressure to perform sensitive and accurate analytical studies to detect, identify, and quantify extractable and leachable compounds (E&Ls)...

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The constant need to develop more rapid and cost-effective technologies for accurate, sensitive and specific detection in biological samples is a driving force behind the integration of new sample preparation tools, automation and informatics across the bioanalytical workflow...

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